Synthetic method of nitrogen-enriched carbon coated lithium titanate composite material prepared by introduction of ionic liquid as carbon source

An ionic liquid and lithium titanate-coated technology, which is applied in electrical components, battery electrodes, circuits, etc., can solve the problems of electrolyte loss, low electronic conductivity of pure-phase lithium titanate, and electrolyte reaction, so as to improve flatulence problem, the effect of excellent rate performance and cycle performance

Inactive Publication Date: 2012-12-12
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most commercial lithium-ion batteries use carbon materials as negative electrode materials, but carbon materials themselves have some disadvantages: (1) SEI film will be formed, and its first charge and discharge efficiency is low; (2) its cut-off potential is close to that of metal lithium, Lithium dendrites will be formed when the battery is overcharged, causing a short circuit and causing safety problems; (3) It has obvious voltage hysteresis; (4) It is easy to react with the electrolyte and cause the loss of the electrolyte; the spinel lithium titanate material is used as Lithium-ion battery anode materials are increasingly valued, and it has incomparable advantages compared with commercial carbon materials: it has a higher Ti 4+ / Ti 3+ (1.55V vs Li + / Li) oxidation-reduction potential, no SEI film will be formed on the surface; it has a spinel structure, and its volume hardly changes during charge and discharge, so it has a cycle life better than that of carbon anode materials; it has a three-dimensional lithium The ion diffusion channel is conducive to the rapid deintercalation reaction of lithium ions, and has excellent high-rate charge and discharge performance; it also has an ideal charge and discharge platform, and has obvious voltage mutation characteristics at the end of charging; its preparation raw materials have a wide range of sources and are clean
[0004] However, the electronic conductivity of pure phase lithium titanate is very low, which affects the charge and discharge performance of lithium ion battery electrode materials, especially its poor fast charge and discharge performance, so it must be modified to achieve the level of use.

Method used

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  • Synthetic method of nitrogen-enriched carbon coated lithium titanate composite material prepared by introduction of ionic liquid as carbon source
  • Synthetic method of nitrogen-enriched carbon coated lithium titanate composite material prepared by introduction of ionic liquid as carbon source
  • Synthetic method of nitrogen-enriched carbon coated lithium titanate composite material prepared by introduction of ionic liquid as carbon source

Examples

Experimental program
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Effect test

Embodiment 1

[0027] a) Weigh lithium carbonate, titanium dioxide and polyvinyl alcohol according to the molar ratio of lithium, titanium and carbon as 4.2:5:0.2, add a certain amount of alcohol and place them in a ball mill for stirring and ball milling. The ball milling time is 5 hours. The finished slurry is placed in a vacuum drying oven for drying treatment at a temperature of 80 degrees and a drying time of 8 hours.

[0028] b) The dried precursor was placed in an atmosphere protection furnace for sintering, and the temperature was raised to 800 °C at a heating rate of 2 °C / min, kept for 12 hours, and naturally cooled to room temperature to obtain a primary carbon-coated lithium titanate material.

[0029] c) Weigh a certain amount of primary carbon-coated lithium titanate material, and weigh 1-ethyl-3-methylimidazolium dicyandiamide salt (EMIM -DCA), add an appropriate amount of deionized water for another ball milling dispersion treatment, add an appropriate amount of deionized wate...

Embodiment 2

[0032] a) Weigh lithium carbonate, titanium dioxide and polyvinyl alcohol according to the molar ratio of lithium, titanium and carbon elements of 4.2:5:0.5, add a certain amount of alcohol and place them in a ball mill for stirring and ball milling. The ball milling time is 8 hours. The finished slurry is placed in a vacuum drying oven for drying treatment at a temperature of 90 degrees and a drying time of 10 hours.

[0033] b) The dried precursor was placed in an atmosphere protection furnace for sintering, and the temperature was raised to 850 °C at a heating rate of 5 °C / min, kept for 12 hours, and naturally cooled to room temperature to obtain a primary carbon-coated lithium titanate material.

[0034] c) Weigh a certain amount of primary carbon-coated lithium titanate material, and weigh 1-ethyl-3-methylimidazolium dicyandiamide salt (EMIM -DCA), adding an appropriate amount of deionized water for another ball milling dispersion treatment, adding an appropriate amount o...

Embodiment 3

[0037] a) Weigh lithium carbonate, titanium dioxide and polyvinyl alcohol according to the molar ratio of lithium, titanium and carbon elements of 4.2:5:0.8, add a certain amount of alcohol and place them in a ball mill for stirring and ball milling. The ball milling time is 10 hours. The finished slurry is placed in a vacuum drying oven for drying treatment at a temperature of 100 degrees and a drying time of 12 hours.

[0038] b) The dried precursor was placed in an atmosphere protection furnace for sintering, and the temperature was raised to 880 °C at a heating rate of 8 °C / min, kept for 12 hours, and naturally cooled to room temperature to obtain a primary carbon-coated lithium titanate material.

[0039] c) Weigh a certain amount of primary carbon-coated lithium titanate material, and weigh 1-ethyl-3-methylimidazolium dicyandiamide salt (EMIM -DCA), adding an appropriate amount of deionized water for another ball milling dispersion treatment, adding an appropriate amount...

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Abstract

The invention discloses a synthetic method of a nitrogen-enriched carbon coated lithium titanate composite material prepared by the introduction of an ionic liquid as a carbon source. The synthetic method comprises the following steps of: 1) weighing lithium salt, titanium dioxide and the carbon source in proportion, adding alcohol, carrying out ball milling dispersion, and carrying out vacuum drying to prepare a precursor; 2) sintering the prepared precursor at the temperature of 750-950 DEG C under the protection of an inert atmosphere so as to preliminarily obtain lithium titanate with a carbon material coated on the surface; and 3) adding the ionic liquid and deionized water in proportion into the preliminarily obtained carbon-coated lithium titanate, carrying out ball milling, stirring and sintering. The lithium titanate composite material has a spherical morphology of nano-primary particle composed micrometer secondary particles, and the surface of the lithium titanate composite material is uniformly coated with a layer of nitrogen-enriched carbon material. Its electronic conductivity is not only effectively raised, but surface stability of the material is also enhanced. The obtained material has excellent rate capability and cycle performance. In addition, gas expansion problem of lithium titanate cells is effectively improved. The nitrogen-enriched carbon coated lithium titanate composite material has a wide application prospect in the field of lithium ion battery.

Description

technical field [0001] The present invention relates to a preparation method of lithium titanate composite material coated with nitrogen-containing carbon as negative electrode material of lithium ion battery, in particular to the method of adopting secondary coating in the material synthesis process and introducing ionic liquid as carbon source to the surface of lithium titanate. Coating treatment is carried out. The coating layer is a nitrogen-containing carbon material, which improves the cycle performance and rate performance of the material, and effectively improves the flatulence problem of the lithium titanate system battery. It belongs to the field of electrochemical material preparation technology and new energy . Background technique [0002] With the environmental problems and energy crisis attracting people's attention day by day, it is imperative to develop clean energy. In the development of new energy, lithium-ion batteries are actively developing in the dire...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M10/42
CPCY02E60/122Y02E60/10
Inventor 杨茂萍杨续来郭钰静王康平谢佳
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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